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Water → HCID 57296520, 화합물

HRID 1905399
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HRID 1905399 반응식
[Cl:1][C:2]1[CH:18]=[CH:17][C:5]([O:6][C:7]2[N:11]([CH3:12])[N:10]=[C:9]([CH3:13])[C:8]=2[CH:14]=[N:15][OH:16])=[CH:4][CH:3]=1.[OH-].[Na+].Br[CH2:22][C:23]1[CH:32]=[CH:31][CH:30]=[CH:29][C:24]=1[C:25]([O:27][CH3:28])=[O:26].O>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([O:6][C:7]2[N:11]([CH3:12])[N:10]=[C:9]([CH3:13])[C:8]=2[CH:14]=[N:15][O:16][CH2:22][C:23]2[CH:32]=[CH:31][CH:30]=[CH:29][C:24]=2[C:25]([O:27][CH3:28])=[O:26])=[CH:17][CH:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 12148555-(4-Chlorophenoxy)-1,3-dimethyl-1H-pyrazole-4-carboxaldehyde oximeHCID 2734813Methyl 2-(bromomethyl)benzoate

생성물 1

HCID 57296520HCID 57296520, 화합물수율 64%

시약·촉매·용매 1

HCID 6228
Dimethylformamide
용매

실험 절차

2.0 Grams (0.00755 mole) of 5-(4-chlorophenoxy)-1,3-dimethyl-pyrazole-4-carbaldehyde oxime was dissolved in 20 ml of dimethylformamide, and after adding 0.5 g (0.0125 mole) of powdery sodium hydroxide, the resulting mixture was thoroughly stirred. To this solution was added 1.73 g (0.00755 mole) of methyl 2-bromomethylbenzoate, and reaction was carried out at from 70° to 80° C. for 5 hours. After completion of the reaction, water was added to the reaction solution which was then extracted with ethyl acetate. The ethyl acetate extract was washed with water and dried, and ethyl acetate was removed by evaporation to obtain an oily product. This oily product was column-chromatographed on silica gel to obtain 2.0 g cf the desired compound.

후처리

  1. additionTo this solution was added
  2. additionwas added to the reaction solution which
  3. extractionwas then extracted with ethyl acetate
  4. extractionThe ethyl acetate extract
  5. washwas washed with water
  6. customdried
  7. customethyl acetate was removed by evaporation
  8. customto obtain an oily product
  9. customThis oily product was column-chromatographed on silica gel

출처 및 근거

ORD 기록
ord-8e2f7b376ba54bddb235da80c47af322
출처 데이터셋
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04843068

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